CN111905820B - 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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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 30
- 239000001301 oxygen Substances 0.000 title claims abstract description 30
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 17
- 229920000620 organic polymer Polymers 0.000 title claims abstract description 16
- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims description 5
- -1 transition metal salt Chemical class 0.000 claims abstract description 36
- 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 15
- 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
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 239000011572 manganese Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 125000006384 methylpyridyl group Chemical group 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 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
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 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
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 claims 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 4
- 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 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
- 239000000446 fuel Substances 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
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 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
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 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
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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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
- B01J31/1691—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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- C08G83/008—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
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- H—ELECTRICITY
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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; and putting the obtained mixture into a polytetrafluoroethylene-lined high-pressure kettle, 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 precipitation reaction. 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 slower than the hydrogen evolution reaction of the cathode by four orders of magnitude, which seriously restricts the hydrogen production efficiency, therefore, the key for improving the whole hydrolysis efficiency is to accelerate the oxygen evolution reaction rate. 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) 2 O) 2 ]·3H 2 Crystal structure diagram of O;
FIG. 2 shows [ Ni (L) (1, 2-BDC) (H) 2 O) 2 ]·3H 2 O is loaded on the oxygen precipitation linear scanning curve of the rotating disk electrode;
FIG. 3 is [ Co (L) (1, 3-BDC) (H) 2 O) 2 ]·3H 2 Crystal structure diagram of O;
FIG. 4 is [ Co (L) (1, 3-BDC) (H) 2 O) 2 ]·3H 2 O is loaded on the oxygen precipitation linear scanning curve of the rotating disk electrode;
FIG. 5 shows [ Mn (L) (2, 5-BDC) (H) 2 O) 2 ]·3H 2 Crystal structure diagram of O;
FIG. 6 shows [ Mn (L) (2, 5-BDC) (H) 2 O) 2 ]·3H 2 O 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 a transition metal containing organic polymer 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 a polytetrafluoroethylene-lined autoclave with the 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 precipitation 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 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 and N, N-bis (amino-piperidyl) -naphthalimide.
Example 1
N, N-bis (methyl-pyrrolyl) -naphthalimide, N-bis (methyl-pyridinyl) -naphthalimide, N-bis (methyl-piperidinyl) -naphthalimide, N-bis (amino-pyrrolyl) -naphthalimide, N-bis (amino-pyridinyl) -naphthalimide, N-bis (amino-piperidinyl) -naphthalimide
[Co(L)(1,2-BDC)(H 2 O) 2 ]·3H 2 And (3) synthesis of O: based on L (N, N-bis (methyl-pyridyl) -naphthalimide) (amount of substance 0.002 mol), coCl 2 ·6H 2 O、L、1,2-H 2 BDC 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) 2 O) 2 ]·3H 2 The crystal structure of O is shown in FIG. 1.
5mg of [ Co (L) (1, 2-BDC) (H) are weighed out 2 O) 2 ]·3H 2 O into a centrifuge tube, adding 0.49mL of deionized water, 0.49mL of absolute ethyl alcohol and 0.02mL of Nafion (5% by mass percent) solution, performing ultrasonic treatment for 30 minutes, sucking 8.3 mu L of the solution by using a pipette, dropping the solution on glassy carbon, and rotating the solutionLinear scan curves for testing on disk electrodes (5 mm diameter) after drying at room temperature in 1M KOH solution saturated with oxygen are shown in figure 2.
Example 2
[Ni(L)(1,3-BDC)(H 2 O) 2 ]·3H 2 And (3) synthesis of O: based on L (N, N-bis (methyl-pyridyl) -naphthalamide) (amount of substance 0.001 mol), ni 2 (CH 3 COO) 2 、L、1,2-H 2 BDC 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) 2 O) 2 ]·3H 2 The crystal structure of O is shown in FIG. 3.
5mg of [ Ni (L) (1, 3-BDC) (H) are weighed out 2 O) 2 ]·3H 2 O 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)(H 2 O) 2 ]·3H 2 And (3) synthesis of O: based on L (N, N-bis (methyl-pyridyl) -naphthalamide) (amount of substance 0.001 mol), mnCl 2 、L、1,2-H 2 BDC and NaOH are respectively 1:1:1:3 and an appropriate amount of deionized water, and the mixture was placed in a 200mL autoclave lined with polytetrafluoroethylene and stored at 120 ℃ for 4 days. After slowly cooling to room temperature, the mixture was filtered, washed and dried to obtain [ Mn (L) (2, 5-BDC) (H) 2 O) 2 ]·3H 2 The 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 (3)
1. The application of an electrocatalyst containing a transition metal organic polymer in an electrolytic water oxygen evolution reaction is characterized in that the preparation method of the electrocatalyst comprises the following steps:
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; the chain naphthalimide is N, N-bi (methyl-pyridyl) -naphthalimide;
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.
2. The use of an electrocatalyst for an organic polymer comprising transition metal(s) according to claim 1 in electrolysis water oxygen evolution reactions, wherein the metal element in the transition metal salt is one or more of cobalt, nickel and manganese.
3. The use of an electrocatalyst for transition metal-containing organic polymers according to claim 1 in electrolysis water oxygen evolution reactions, wherein the transition metal salt is one or more of transition metal chloride, transition metal acetate, transition metal nitrate.
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| WO2020073398A1 (en) * | 2018-10-09 | 2020-04-16 | 苏州大学 | Ultrathin ni-fe-mof nanosheet, preparation method therefor and application thereof |
| CN111111716A (en) * | 2020-01-19 | 2020-05-08 | 西北师范大学 | Preparation and application of nickel-cobalt double-metal phosphide guided by MOF |
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