CN109453813A - A kind of preparation method of low cost and efficient iron series oxygen reduction reaction catalyst - Google Patents
A kind of preparation method of low cost and efficient iron series oxygen reduction reaction catalyst Download PDFInfo
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- CN109453813A CN109453813A CN201811408965.9A CN201811408965A CN109453813A CN 109453813 A CN109453813 A CN 109453813A CN 201811408965 A CN201811408965 A CN 201811408965A CN 109453813 A CN109453813 A CN 109453813A
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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
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2217—At least one oxygen and one nitrogen atom present as complexing atoms in an at least bidentate or bridging ligand
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a kind of low cost and the preparation methods of efficient iron series oxygen reduction reaction catalyst.(1) in 50 DEG C of -80 DEG C of temperature ranges, betanaphthol is dissolved in sodium hydroxide solution, after dissolution completely, sodium nitrite is added in above-mentioned betanaphthol mixed solution, nitroso-beta-naphthol mixed solution i.e. NOL is synthesized;(2) ferric ion solutions are prepared with Fe(NO3)39H2O;(3) NOL is slowly added into ferric ion solutions, is stirred to react, dry to obtain NOL-Fe.(4) NOL-Fe, urea and carbon black are dissolved in dehydrated alcohol, dried, and be activated under nitrogen atmosphere protection, be cooled to room temperature, obtain iron series oxygen reduction reaction catalyst.Manufacturing process of the present invention is simple and at low cost, the obvious superior Pt/C catalyst of the redox reactions catalytic performance and stability of activation products, it is possible to will become the candidate of oxygen reduction catalyst agent on fuel cell and metal air battery cathodes.
Description
Technical field
The present invention relates to a kind of low cost and the preparation methods of efficient iron series oxygen reduction reaction catalyst.
Background technique
Fossil energy if being widely used for petroleum, natural gas and coal has pushed the fast development of human society, but is changed
The non-renewable and use process bring environmental problem of the stone energy is two hang-ups of facing mankind.Develop environment friend
Oneself is become the mostly important research hotspot in the world today for good, reproducible new energy and new energy technology, causes that people's is wide
General concern.Fuel cell be it is a kind of without burning directly by chemical energy be converted into electric energy novel energy converting system and other
New energy technology is compared, and has energy transition density high, pollutes small, fuel diversification, high reliablity, low noise and convenient for safeguarding
The advantages that, it is widely regarded as most possibly obtaining the new energy technology of large-scale commercial application.But fuel cell is high
Manufacturing cost be always to hinder the barrier of its commercialized development.Platinum based catalyst used in fuel cell be cause it high at
One of this main reason for, in particular for the platinum group cathod catalyst of Cathodic oxygen reduction.Due to the yin of oxygen reduction reaction
Pole kinetics process opposite anode hydroxide process is more slow and complicated, therefore the carrying capacity of required platinum is bigger, for this purpose, replacing
Become the important directions of fuel cell for the research and development of the non noble metal oxygen reduction catalyst of noble metal.
Currently, including that M-N-C(M represents transition metal element) type nitrating C catalyst, transition metal macrocyclic compound, mistake
The non-precious metal catalyst for crossing metal oxide, transition metal nitride and the polymer without coordinating metal receives extensive pass
Note and further investigation, but wherein, the catalytic activity of transition metal oxide and transition metal nitride class is relatively low, and M-N-C type
Nitrating C catalyst receives sizable pass because of activity higher under its cheap cost, acidic environment and outstanding stability
Note.Develop significantly although the cost control and preparation method about M-N-C type catalyst have had, current system
The Preparation Method universal test period is long, energy consumption is high, poisonous and harmful, is unfavorable for being mass produced.Transition metal macrocyclic compound has
Higher initial catalytic activity, wherein macrocyclic compound presoma be mainly with conductive compounds such as porphyrin, pyridine, phthalocyanines
The disadvantages of master, generally stability is poor in acid condition for they, and there are expensive raw material prices, this promotes still commercialization
There have to be very big unfavorable.
Therefore, need to develop that a kind of process flow is simple, presoma is at low cost, synthetic product has high activity and goes out at present
The preparation method of the transition metal chelate oxygen reduction reaction catalyst of color stability.
Summary of the invention
It is low the object of the present invention is to provide a kind of synthesis cost and with efficient and stable oxygen reduction reaction catalyst
Preparation method.
Specific steps are as follows:
(1) in 50 DEG C of -80 DEG C of temperature ranges, the betanaphthol of 5-10 g, which is dissolved in 100-200 mL mass percent concentration, is
In the sodium hydroxide solution of 1-5%, after dissolution completely, sodium nitrite is by betanaphthol: the molal weight ratio of sodium nitrite is in terms of 1:1
Amount synthesizes 0.1-1mol/L alpha-nitroso-beta-naphthol mixed solution i.e. according to being added in above-mentioned betanaphthol mixed solution
NOL。
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into 0.1-1mol/L ferric ion solutions.
(3) it is 1:3 with Fe:NOL molar ratio, the mixed solution that step (1) synthesizes is slowly added into step (2) preparation
In ferric ion solutions, be arranged 50-80 DEG C of temperature range water-bath in be stirred to react 3 hours, product is filtered and spend from
It is dried after sub- water washing at 80 DEG C, obtains iron series oxygen reduction reaction catalyst precursor and be denoted as NOL-Fe, iron series oxygen reduction reaction is urged
Agent presoma can be directly tested for the property.
(4) NOL-Fe, 4-7g urea of 0.5-2g and 0.1g carbon black are dissolved in 100-500 mL dehydrated alcohol, then dried
It is dry, obtain mixed-powder, and under nitrogen atmosphere protection, 800 DEG C activation processing 1-2 hours, then naturally cool to room temperature, obtain
Iron series oxygen reduction reaction catalyst, then carry out redox reactions performance test.
The monomer that betanaphthol of the present invention is made of double phenyl ring and monohydroxy is among a kind of widely used organic chemical industry
Body, raw material are easy to get, moderate.In addition, betanaphthol is can be used as in non-ferrous metal metallurgy technique except ferron, betanaphthol is first
It is reacted with sodium nitrite and synthesizes alpha-nitroso-beta-naphthol, then reacted with iron ion, synthesis alpha-nitroso-beta-naphthol iron chelating
Object, the thermal decomposition product mixed with urea, carbon black are possible to that the cathode catalyst materials quotient such as fuel cell, air cell will be become
The accelerator of industryization application.Synthesis technology of the present invention is simple, at low cost, is a kind of catalyst synthesis with preferable application prospect
Method.
Detailed description of the invention
Fig. 1 is the shape appearance figure of NOL-Fe presoma made from 1-2 of the embodiment of the present invention.
Fig. 2 is NOL-Fe presoma cyclic voltammetry curve figure made from 1-2 of the embodiment of the present invention.
Fig. 3 is NOL-Fe presoma linear sweep voltammetry curve graph made from 1-2 of the embodiment of the present invention.
Fig. 4,5 are the cyclic voltammetric of the iron series oxygen reduction reaction catalyst prepared under 3-5 of embodiment of the present invention different condition
Curve graph.
Fig. 6,7 are the linear scan of the iron series oxygen reduction reaction catalyst prepared under 3-5 of embodiment of the present invention different condition
Volt-ampere curve figure.
Fig. 8 is the stability curve figure of the iron series oxygen reduction reaction catalyst of 3-5 of embodiment of the present invention preparation.
Specific embodiment
Embodiment 1:
In (1) 60 DEG C of temperature range, it is molten that the betanaphthol of 5 g is dissolved in the sodium hydroxide that 150 mL mass percent concentrations are 1%
In liquid, after dissolution completely, 2.4 g sodium nitrites is added, synthesize 0.6 mol/L alpha-nitroso-beta-naphthol mixed solution.
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into the solution i.e. NOL that iron ion is 0.2 mol/L.
(3) it is 1:3 metering with Fe:NOL molar ratio, the mixed solution that step (1) synthesizes is slowly added into step (2) and is matched
In the ferric ion solutions of system, it is stirred to react in the water-bath of 60 DEG C of temperature ranges 3 hours, product is filtered and uses deionized water
It is dried after washing at 80 DEG C, obtains iron series oxygen reduction reaction catalyst precursor and be denoted as NOL-Fe.
(4) NOL-Fe that step (3) make directly is subjected to redox reactions performance test, and is urged with commercialization Pt/C
Agent comparison.The pattern of NOL-Fe sample is shown in Fig. 1, and hydrogen reduction catalytic performance test result is shown in attached drawing 2 and Fig. 3.
Embodiment 2:
In (1) 50 DEG C of temperature range, it is molten that the betanaphthol of 10 g is dissolved in the sodium hydroxide that 200 mL mass percent concentrations are 2%
In liquid, after dissolution completely, with betanaphthol: sodium nitrite molal weight ratio is that 1:1 payment foundation weighs sodium nitrite, is added to
It states in betanaphthol mixed solution, synthesizes the 0.3 i.e. NOL of mol/L alpha-nitroso-beta-naphthol mixed solution.
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into the solution that iron ion is 0.1 mol/L.
(3) it is 1:3 metering with Fe:NOL molar ratio, the mixed solution that step (1) synthesizes is slowly added into step (2) and is matched
In the ferric ion solutions of system, it is stirred to react in the water-bath of 60 DEG C of temperature ranges 3 hours.Product is filtered and uses deionized water
It is dried after washing, obtains iron series oxygen reduction reaction catalyst precursor and be denoted as NOL-Fe.
(4) NOL-Fe that step (3) make directly is subjected to redox reactions performance test, and is urged with commercialization Pt/C
Agent comparison.The pattern of NOL-Fe sample is shown in Fig. 1, and hydrogen reduction catalytic performance test result is shown in attached drawing 2 and Fig. 3.
Embodiment 3:
In (1) 60 DEG C of temperature range, it is molten that the betanaphthol of 10 g is dissolved in the sodium hydroxide that 200 mL mass percent concentrations are 3%
In liquid, after dissolution completely, with betanaphthol: sodium nitrite molal weight ratio is that 1:1 payment foundation weighs sodium nitrite, is added to
It states in betanaphthol mixed solution, synthesizes the 0.3 i.e. NOL of mol/L alpha-nitroso-beta-naphthol mixed solution.
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into the solution that iron ion is 0.1 mol/L.
(3) it is 1:3 metering with Fe:NOL molar ratio, the mixed solution that step (1) synthesizes is slowly added into step (2) and is matched
In the ferric ion solutions of system, it is stirred to react in the water-bath of 60 DEG C of temperature ranges 3 hours.Product is filtered and uses deionized water
It is dried after washing at 80 DEG C, obtains iron series oxygen reduction reaction catalyst precursor and be denoted as NOL-Fe.
(4) it takes 0.1g NOL-Fe, 6g urea and 0.1g carbon black to be dissolved in 100 mL dehydrated alcohols, then dries, obtain
Mixed-powder, and under nitrogen atmosphere protection, in 800 DEG C of progress high-temperature activations, 2 hours are kept the temperature, then naturally cool to room temperature, obtained
Iron series oxygen reduction reaction catalyst, finally to iron series oxygen reduction reaction catalyst carries out redox reactions performance and stabilization
Performance test, and with commercialization Pt/C COMPARATIVE CATALYST, test result is shown in attached drawing 4, Fig. 5, Fig. 6, Fig. 7 and Fig. 8.
Embodiment 4:
In (1) 60 DEG C of temperature range, it is molten that the betanaphthol of 10 g is dissolved in the sodium hydroxide that 200 mL mass percent concentrations are 4%
In liquid, after dissolution completely, with betanaphthol: sodium nitrite molal weight ratio is that 1:1 payment foundation weighs sodium nitrite, is added to
It states in betanaphthol mixed solution, synthesizes the 0.3 i.e. NOL of mol/L alpha-nitroso-beta-naphthol mixed solution.
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into the solution that iron ion is 0.1 mol/L.
(3) it is 1:3 metering with Fe:NOL molar ratio, the mixed solution that step (1) synthesizes is slowly added into step (2) and is matched
In the ferric ion solutions of system, it is stirred to react in the water-bath of 60 DEG C of temperature ranges 3 hours.Product is filtered and uses deionized water
It is dried after washing at 80 DEG C, obtains iron series oxygen reduction reaction catalyst precursor and be denoted as NOL-Fe.
(4) it takes 0.15g NOL-Fe, 5g urea and 0.1g carbon black to be dissolved in 150 mL dehydrated alcohols, then dries, obtain
Mixed-powder, and under nitrogen atmosphere protection, it is heat-treated at 800 DEG C, keeps the temperature 2 hours, then naturally cool to room temperature, obtain iron
It is oxygen reduction reaction catalyst, finally to the progress redox reactions performance test of iron series oxygen reduction reaction catalyst is obtained, tests
The results are shown in attached figure 4, Fig. 5, Fig. 6 and Fig. 7.
Embodiment 5:
In (1) 60 DEG C of temperature range, it is molten that the betanaphthol of 10 g is dissolved in the sodium hydroxide that 200 mL mass percent concentrations are 5%
In liquid, after dissolution completely, with betanaphthol: sodium nitrite molal weight ratio is that 1:1 payment foundation weighs sodium nitrite, is added to
It states in betanaphthol mixed solution, synthesizes the 0.3 i.e. NOL of mol/L alpha-nitroso-beta-naphthol mixed solution.
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into the solution that iron ion is 0.1 mol/L.
(3) it is 1:3 metering with Fe:NOL molar ratio, the mixed solution that step (1) synthesizes is slowly added into step (2) and is matched
In the ferric ion solutions of system, it is stirred to react in the water-bath of 60 DEG C of temperature ranges 3 hours.Product is filtered and uses deionized water
It is dried after washing at 80 DEG C, obtains iron series oxygen reduction reaction catalyst precursor and be denoted as NOL-Fe.
(4) it takes 0.2g NOL-Fe and 4g urea and 0.1g carbon black to be dissolved in 200 mL dehydrated alcohols, then dries, obtain
Mixed-powder, and under nitrogen atmosphere protection, it is heat-treated at 800 DEG C, keeps the temperature 2 hours, then naturally cool to room temperature, obtain iron
It is oxygen reduction reaction catalyst, finally to the progress redox reactions performance test of iron series oxygen reduction reaction catalyst is obtained, tests
The results are shown in attached figure 4, Fig. 5, Fig. 6 and Fig. 7.
It is pointed out that technical solution according to the invention, above-described embodiment can also enumerate many, according to applicant
A large amount of the results show can achieve the purpose of the present invention in the range that claims of the present invention is proposed.
Claims (1)
1. the preparation method of a kind of low cost and efficient iron series oxygen reduction reaction catalyst, it is characterised in that specific steps are as follows:
(1) in 50 DEG C of -80 DEG C of temperature ranges, the betanaphthol of 5-10 g, which is dissolved in 100-200 mL mass percent concentration, is
In the sodium hydroxide solution of 1-5%, after dissolution completely, sodium nitrite is by betanaphthol: the molal weight ratio of sodium nitrite is in terms of 1:1
Amount synthesizes 0.1-1mol/L alpha-nitroso-beta-naphthol mixed solution i.e. according to being added in above-mentioned betanaphthol mixed solution
NOL;
(2) it is mixed with Fe(NO3)39H2O with deionized water, is made into 0.1-1mol/L ferric ion solutions;
(3) be 1:3 with Fe:NOL molar ratio, by step (1) synthesize mixed solution be slowly added into step (2) preparation iron from
In sub- solution, it is stirred to react 3 hours in the water-bath that 50-80 DEG C of temperature range is set, product is filtered and uses deionized water
It is dried after washing at 80 DEG C, obtains iron series oxygen reduction reaction catalyst precursor material NOL-Fe;
(4) NOL-Fe, 4-7g urea of 0.5-2g and 0.1g carbon black are dissolved in 100-500 mL dehydrated alcohol, then dried,
Obtain mixed-powder, and under nitrogen atmosphere protection, 800 DEG C activation processing 1-2 hours, then naturally cool to room temperature, obtain iron
It is oxygen reduction reaction catalyst.
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CN111408369A (en) * | 2020-04-16 | 2020-07-14 | 桂林理工大学 | Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof |
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CN103747872A (en) * | 2011-08-08 | 2014-04-23 | 昭和电工株式会社 | Method for producing redox catalyst and use of redox catalyst |
CN106831431A (en) * | 2017-02-20 | 2017-06-13 | 桂林理工大学 | The preparation method of low-cost high-efficiency oxygen reduction reaction α nitroso Beta Naphthol 99MIN cobalt chelates and the application as catalyst |
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