CN109926095A - Cobalt-based oxygen-separating catalyst, preparation method and its electro-catalysis based on eutectic solvent analyse oxygen application - Google Patents
Cobalt-based oxygen-separating catalyst, preparation method and its electro-catalysis based on eutectic solvent analyse oxygen application Download PDFInfo
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Abstract
The present invention provides a kind of cobalt-based oxygen-separating catalyst based on eutectic solvent, preparation method and its electro-catalysis analysis oxygen application.The preparation method of catalyst of the present invention, comprising steps of (1) mixes cobalt chloride hexahydrate and urea, it is stirred at 70-90 DEG C, obtain eutectic solvent, eutectic solvent is reacted at 150-200 DEG C, it is cooled to room temperature after completion of the reaction, obtained solid is washed, is dried to obtain cobalt amine complex；(2) the cobalt amine complex for obtaining step (1) is modified in nickel foam, is activated using chronoamperometry to it, is obtained cobalt-based oxygen-separating catalyst in foam nickel surface.Gained cobalt-based oxygen-separating catalyst of the invention is sheet-like morphology, has excellent analysis oxygen catalytic performance and splendid stability.The present invention prepares cobalt-based oxygen-separating catalyst using eutectic solvent, and preparation process is simple, low in cost, environmentally protective, is suitble to large-scale production.
Description
Technical field
The present invention relates to a kind of, and cobalt-based oxygen-separating catalyst, preparation method and its electro-catalysis analysis oxygen based on eutectic solvent are answered
With belonging to field of energy source materials.
Background technique
Hydrogen is a kind of novel clean energy resource, can replace traditional fossil energy, to alleviate energy shortages and environment
The problems such as pollution.Hydrogen has many sources, and wherein electro-catalysis water-splitting is to prepare one of important method of hydrogen, electro-catalysis water crack
Solution includes two half-reactions, respectively evolving hydrogen reaction and oxygen evolution reaction.Wherein, oxygen evolution reaction mechanism is more complex, the electrode needed
Overpotential is larger, and more electric energy is lost, in order to reduce the overpotential of oxygen evolution reaction, it would be desirable to synthesize oxygen-separating catalyst.Mesh
In preceding common oxygen-separating catalyst, with rhodium metal catalyst, iraurite metal catalyst is that the catalysis of the noble metal catalyst of representative is living
Property highest, stability is best, however due to its rare deposit and expensive price, and noble metal catalyst can not be applied to big rule
In the industrial production of mould.Therefore, it is badly in need of a kind of inexpensive, efficient oxygen-separating catalyst.
Transition metal such as cobalt, nickel, iron, since it contains the d track and unpaired electron of underfill, catalytic activity is good,
Therefore transition-metal catalyst is the good substitute of noble metal catalyst, is expected to electro-catalysis water-splitting hydrogen manufacturing putting into big rule
In mould industrial production.Wherein, the one kind of cobalt-base catalyst as transition-metal catalyst shows good catalytic performance.
Many patent documents that are prepared with about cobalt-base catalyst are reported, for example, Chinese patent document CN107308958A is mentioned
A kind of preparation method of oxygen evolution reaction electrochemical catalyst is supplied, comprising the following steps: 1) by cobalt salt and non-ionic surface active
Agent polymer, which is added to the water, to be stirred and evenly mixed, and hydrazine hydrate is then added, and hatches obtain lamella cobalt hydroxide under hydrothermal conditions, and 2)
Obtained lamella cobalt hydroxide and Thiomolybdate are added in n,N-Dimethylformamide, then ultrasonic disperse mixing exists
It is pyrolyzed Thiomolybdate under the conditions of solvent heat, obtains the vulcanization molybdenum layer of amorphous phase on the surface of lamella substrate.But this method obtains
The oxygen-separating catalyst arrived is in 10mA/cm2Current density under, overpotential can be up to 350mV or more, and overpotential is higher,
More electric energy is lost.Chinese patent document CN107486233A discloses a kind of carbon-based cobalt/cobalt oxide nanometer of carbonitride doping and urges
The alkaline solution of the raw material and dicyandiamide that prepare MOF is blended and gel is made by the preparation method of agent, main preparation step,
It is isolated obtained MOF dicyandiamide nanocrystal, it is heated in air atmosphere, carbonitride is made and adulterates carbon-based cobalt oxidation
Object nanocatalyst.But the preparation method is more complicated, higher cost.
Therefore, the industrial cost of hydrogen is produced in order to reduce water-splitting, the cobalt-base catalyst of synthesis there need to be following characteristics:
(1) simple synthetic method, low in cost, pollution-free and toxicity；(2) surface area of catalyst should be big as far as possible, more with exposure
Catalytic site enhances its catalytic activity, and this requires the catalyst morphologies of synthesis should be sheet or the knot of other large specific surface areas
Structure.But the cobalt-base catalyst reported at present cannot be considered in terms of the above two o'clock mostly, this strongly limits electro-catalysis water-splitting industry
The application of change.
Summary of the invention
In view of the deficiencies of the prior art, the cobalt-based oxygen-separating catalyst that the present invention provides a kind of based on eutectic solvent, system
Oxygen application is analysed in Preparation Method and its electro-catalysis.Preparation method of the invention is low in cost, easy, meets the atom economy of Green Chemistry
Theory.
Technical scheme is as follows:
A kind of cobalt-based oxygen-separating catalyst based on eutectic solvent, the catalyst are in cobalt chloride hexahydrate and urea structure
At eutectic solvent in be prepared；The pattern of the catalyst is sheet, granularity 400-600nm.
According to the present invention, the preparation method of the above-mentioned cobalt-based oxygen-separating catalyst based on eutectic solvent, comprises the following steps that
(1) cobalt chloride hexahydrate and urea are mixed, is stirred at 70-90 DEG C, obtain eutectic solvent, by eutectic solvent
It is reacted at 150-200 DEG C；It is cooled to room temperature after completion of the reaction, obtained solid is washed, is dried to obtain cobalt amine complex；
(2) the cobalt amine complex for obtaining step (1) is modified in nickel foam, is activated using chronoamperometry to it,
Foam nickel surface obtains cobalt-based oxygen-separating catalyst.
Preparation method according to the present invention, it is preferred that the molar ratio of cobalt chloride hexahydrate and urea described in step (1)
For 1:(2-4), further preferred 1:(3.5-4).
Preparation method according to the present invention, it is preferred that whipping temp described in step (1) is 80 DEG C, and mixing time is
4-10min。
Preparation method according to the present invention, it is preferred that reaction temperature described in step (1) is 180 DEG C；The reaction
Time is 18-24h, further preferred 21h.
Preparation method according to the present invention, it is preferred that reaction described in step (1) is the height carried out in closed container
Temperature reaction.
Preparation method according to the present invention, it is preferred that washing is washed 3 times with dehydrated alcohol described in step (1)；It is described
Drying is to be dried in vacuo 10-30h at 30-40 DEG C.
According to the present invention, the pattern for the cobalt amine complex that step (1) obtains is porous flake, and the size in hole is 30-
100nm。
Preparation method according to the present invention, it is preferred that modification step described in step (2) are as follows: obtain step (1)
Cobalt amine complex is uniformly mixed with the Nafion reagent of dehydrated alcohol, distilled water and 5wt%, and suspension is made, suspension is repaired
For decorations in nickel foam, the modification amount of the cobalt amine complex is 0.4-0.6mg/cm2；
It is further preferred that the ratio between the quality and the volume of dehydrated alcohol of the cobalt amine complex are (8-12): 1mg/
ML, the ratio between the dehydrated alcohol, volume of distilled water and Nafion reagent are 1:1:0.08.
Preparation method according to the present invention, it is preferred that the condition of chronoamperometry described in step (2) are as follows: utilize occasion
Magnificent CHI 760E electrochemical workstation is modified with the nickel foam of cobalt amine complex as working electrode, saturated calomel electrode conduct
Reference electrode, carbon-point are used as to electrode, and the KOH solution of 1mol/L is electrolyte, and the voltage that chronoamperometry applies is 1.56V.
Preparation method according to the present invention, it is preferred that activation time described in step (2) is 20-24h, further excellent
Select 22h.
According to the present invention, oxygen application is analysed in the electro-catalysis of the above-mentioned cobalt-based oxygen-separating catalyst based on eutectic solvent, is applied to
Electro-catalysis water crack parses oxygen；Preferably, as water-splitting oxygen-separating catalyst, it is applied to photoelectrocatalysis, basic hydrolysis hydrogen occurs
Device or APE hydrolyze battery.
It technical characterstic of the invention and has the beneficial effect that:
1, the present invention is mixed to get eutectic solvent using cobalt source and urea, then obtains eutectic solvent heating reaction
Cobalt amine complex is activated to obtain cobalt-base catalyst by cobalt amine complex using chronoamperometry.The raw materials used in the present invention is inexpensively easy
, preparation process is simple, and it is low in cost, it is environmentally protective, it is suitble to large-scale production.
2, for the present invention using the eutectic solvent of synthesis as whole reactants, the cobalt amine complex obtained after heating can
To analyse oxygen for electro-catalysis, meet the atom economy theory of Green Chemistry.
3, eutectic solvent is prepared using simple method in the present invention, and the eutectic solvent of preparation has template effect,
Catalyst morphology growth can be regulated and controled, catalyst is promoted to form sheet-like morphology, the electrochemistry of catalyst can be improved in sheet-like morphology
Analyse oxygen performance.
4, the cobalt-based oxygen-separating catalyst for the sheet that the present invention is prepared has excellent catalytic electrolysis elutriation oxygen performance, answers
For catalytic electrolysis elutriation oxygen, activity is high, experiments have shown that being 10mA/cm in current density2When, needed for overpotential be only
291mV illustrates that catalytic activity is higher；And experiments have shown that catalyst prepared by the present invention has splendid stability.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrogram of cobalt amine complex prepared by embodiment 1.
Fig. 2 is the X-ray diffraction spectrogram of cobalt-based oxygen-separating catalyst prepared by embodiment 1.
Fig. 3 is the transmission electron microscope photo of cobalt amine complex prepared by embodiment 1, and wherein a is low power number cobalt amine complex
Transmission electron microscope photo, b are the transmission electron microscope photo of high magnification numbe cobalt amine complex.
Fig. 4 is the transmission electron microscope photo of cobalt-based oxygen-separating catalyst prepared by embodiment 1, and wherein a is that low power number cobalt-based analyses oxygen
The transmission electron microscope photo of catalyst, b are the transmission electron microscope photo of high magnification numbe cobalt-based oxygen-separating catalyst.
Fig. 5 is the catalytic electrolysis elutriation oxygen performance test of cobalt amine complex and cobalt-based oxygen-separating catalyst prepared by embodiment 1
Figure.
Fig. 6 is the catalytic electrolysis elutriation oxidative stability figure of cobalt-based oxygen-separating catalyst prepared by embodiment 1.
Fig. 7 is the catalytic electrolysis elutriation oxygen performance test figure of cobalt-based oxygen-separating catalyst prepared by comparative example 1.
Specific embodiment
The present invention is described further combined with specific embodiments below, but not limited to this.
Experimental method described in embodiments following simultaneously is unless otherwise specified conventional method；The reagent and material
Material, unless otherwise specified, commercially obtains.
Embodiment 1
A kind of preparation method of the cobalt-based oxygen-separating catalyst based on eutectic solvent, comprises the following steps that
(1) 1.19g cobalt chloride hexahydrate and 1.10g urea are mixed in beaker, stir 5min under 80 DEG C of water-baths, obtains
To blue eutectic solvent, blue eutectic solvent is transferred in reaction kettle, reacts 21h at 180 DEG C；After the reaction was completed,
Reaction kettle is put into cold water and is cooled to room temperature, red brown solid product is obtained；Obtained solid product is washed with dehydrated alcohol
It washs 3 times, is subsequently placed into vacuum oven, it is 24 hours dry at 30 DEG C, obtain cobalt amine complex；
(2) the cobalt amine complex that step (1) obtains is mixed with the Nafion reagent of dehydrated alcohol, distilled water and 5wt%
Uniformly, suspension is made, by suspension modification in nickel foam, the modification amount of the cobalt amine complex is 0.5mg/cm2；Cobalt ammonia
The ratio between quality and the volume of dehydrated alcohol of complex are 10:1mg/mL, the volume of dehydrated alcohol, distilled water and Nafion reagent
The ratio between be 1:1:0.08；Using occasion China CHI 760E electrochemical workstation, to be modified with the nickel foam of cobalt amine complex as work
Make electrode, as reference electrode, carbon-point is used as to electrode saturated calomel electrode, and the KOH solution of 1mol/L is electrolyte, timing electricity
The voltage that stream method applies is 1.56V, and cobalt amine complex is activated 22h, obtains cobalt-based oxygen-separating catalyst in foam nickel surface.
The X-ray diffraction spectrogram of cobalt amine complex manufactured in the present embodiment is as shown in Figure 1, as can be seen from Figure 1 closed
At substance crystallization it is good, structural formula be [Co (NH3)4CO3]Cl。
The X-ray diffraction spectrogram of cobalt-based oxygen-separating catalyst manufactured in the present embodiment is as shown in Fig. 2, as can be seen from Figure 2
Cobalt-based oxygen-separating catalyst is unformed substance.
The transmission electron microscope photo of cobalt amine complex manufactured in the present embodiment is as shown in figure 3, from figure 3, it can be seen that gained
The pattern of cobalt amine complex is porous flake, and the size in hole is 30-100nm.
The transmission electron microscope photo of cobalt-based oxygen-separating catalyst manufactured in the present embodiment as shown in figure 4, figure 4, it is seen that
The pattern of gained cobalt-based oxygen-separating catalyst is sheet, and granularity is 500nm or so.
Cobalt amine complex manufactured in the present embodiment and cobalt-based oxygen-separating catalyst are carried out to the survey of catalytic electrolysis elutriation oxygen performance
Examination, the specific method is as follows: the electrochemical workstation model occasion China CHI 760E used, wherein using nickel foam as working electrode,
Saturated calomel electrode is reference electrode, and carbon-point is to electrode, and the KOH solution of 1mol/L is electrolyte.It is carried out using polarization curve
Electro-chemical test, voltage 1.2-1.8V, sweep speed 5mV/s.
Used nickel foam working electrode is handled as follows:
A. nickel foam is placed in the hydrochloric acid of 1mol/L, ultrasonic 10min, to remove oxide on surface；Then with distillation
Water and dehydrated alcohol difference ultrasound 10min；Room temperature in vacuo is dry for 24 hours.
B. cobalt-based oxygen-separating catalyst 5mg manufactured in the present embodiment is taken, with 0.5mL distilled water, 0.5mL dehydrated alcohol, 40 μ
The Nafion reagent of L5wt% is uniformly mixed, and is ultrasonically treated 20min, prepares electrode modification liquid.
C. above-mentioned decorating liquid is uniformly applied to foam nickel surface, the modification amount of cobalt-based oxygen-separating catalyst is 0.5mg/cm2。
The catalytic electrolysis elutriation oxygen performance test figure of cobalt amine complex and cobalt-based oxygen-separating catalyst manufactured in the present embodiment is such as
Shown in Fig. 5, from figure 5 it can be seen that being 10mA/cm in current density2, the overpotential of cobalt amine complex is 321mV, cobalt-based analysis
The overpotential of VPO catalysts is 291mV, illustrates that the cobalt-based oxygen-separating catalyst catalytic performance of this implementation preparation is higher.
Cobalt-based oxygen-separating catalyst manufactured in the present embodiment is subjected to catalytic electrolysis elutriation oxygen 12h, catalytic stability such as Fig. 6
It is shown, from fig. 6, it can be seen that being 15mA/cm in current density2When, it can be held essentially constant in 12h current density, illustrate this
The cobalt-based oxygen-separating catalyst performance of invention preparation is stablized.
Embodiment 2
A kind of preparation method of the cobalt-based oxygen-separating catalyst based on eutectic solvent, comprises the following steps that
(1) 1.19g cobalt chloride hexahydrate and 0.90g urea are mixed in beaker, stir 5min under 80 DEG C of water-baths, obtains
To blue eutectic solvent, blue eutectic solvent is transferred in reaction kettle, reacts 21h at 180 DEG C；After the reaction was completed,
Reaction kettle is put into cold water and is cooled to room temperature, red brown solid product is obtained；Obtained product is washed 3 with dehydrated alcohol
It is secondary, it is subsequently placed into vacuum oven, it is 24 hours dry at 40 DEG C, obtain cobalt amine complex；
(2) with described in 1 step of embodiment (2).
Embodiment 3
A kind of preparation method of the cobalt-based oxygen-separating catalyst based on eutectic solvent, comprises the following steps that
(1) 1.19g cobalt chloride hexahydrate and 1.10g urea are mixed in beaker, stir 5min under 80 DEG C of water-baths, obtains
To blue eutectic solvent, blue eutectic solvent is transferred in reaction kettle, reacts 21h at 150 DEG C；After the reaction was completed,
Reaction kettle is put into cold water and is cooled to room temperature, red brown solid product is obtained；Obtained product is washed 3 with dehydrated alcohol
It is secondary, it is subsequently placed into vacuum oven, it is 24 hours dry at 40 DEG C, obtain cobalt amine complex；
(2) with described in 1 step of embodiment (2).
Comparative example 1
A kind of preparation method of cobalt-based oxygen-separating catalyst, comprises the following steps that
(1) 1.19g cobalt chloride hexahydrate and 1.10g urea are mixed in beaker, stir 5min under 80 DEG C of water-baths, obtains
To blue eutectic solvent, blue eutectic solvent is transferred in reaction kettle, reacts 10h at 180 DEG C；After the reaction was completed,
Reaction kettle is put into cold water and is cooled to room temperature, red brown solid product is obtained；Obtained product is washed 3 with dehydrated alcohol
It is secondary, it is subsequently placed into vacuum oven, it is 24 hours dry at 30 DEG C, obtain cobalt amine complex；
(2) with described in 1 step of embodiment (2).
The catalytic electrolysis elutriation oxygen performance test figure of the cobalt-based oxygen-separating catalyst of this comparative example preparation is as shown in fig. 7, from Fig. 7
In as can be seen that current density be 10mA/cm2, the overpotential of cobalt amine complex is 355mV, is much higher than the embodiment of the present invention
1, illustrate that catalyst prepared by the present invention can effectively reduce overpotential, catalytic electrolysis elutriation oxygen activity with higher.
Comparative example 2
A kind of preparation method of cobalt-based oxygen-separating catalyst, comprises the following steps that
1.46g cabaltous nitrate hexahydrate and 1.10g urea are mixed in beaker, 5min is stirred under 80 DEG C of water-baths, not
To eutectic solvent.
Thus comparative example is it is found that eutectic solvent, Jin Erjin can be just prepared in only specific cobalt salt and urea mixing
The oxygen-separating catalyst that one step is prepared pattern of the present invention and has excellent performance.
Claims (10)
1. a kind of cobalt-based oxygen-separating catalyst based on eutectic solvent, which is characterized in that the catalyst is in six chloride hydrates
It is prepared in the eutectic solvent that cobalt and urea are constituted；The pattern of the catalyst is sheet, granularity 400-600nm.
2. the preparation method of the cobalt-based oxygen-separating catalyst described in claim 1 based on eutectic solvent, comprises the following steps that
(1) cobalt chloride hexahydrate and urea are mixed, is stirred at 70-90 DEG C, obtain eutectic solvent, eutectic solvent is existed
It is reacted at 150-200 DEG C；It is cooled to room temperature after completion of the reaction, obtained solid is washed, is dried to obtain cobalt amine complex；
(2) the cobalt amine complex for obtaining step (1) is modified in nickel foam, is activated using chronoamperometry to it, in foam
Nickel surface obtains cobalt-based oxygen-separating catalyst.
3. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that described in step (1)
The molar ratio of cobalt chloride hexahydrate and urea is 1:(2-4), preferably 1:(3.5-4).
4. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that described in step (1)
Whipping temp is 80 DEG C, mixing time 4-10min.
5. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that described in step (1)
Reaction temperature is 180 DEG C；The reaction time is 18-24h, preferably 21h.
6. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that step is washed described in (1)
Wash is washed 3 times with dehydrated alcohol；The drying is to be dried in vacuo 10-30h at 30-40 DEG C.
7. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that described in step (2)
Modification step are as follows: mix the cobalt amine complex that step (1) obtains with the Nafion reagent of dehydrated alcohol, distilled water and 5wt%
Uniformly, suspension is made, by suspension modification in nickel foam, the modification amount of the cobalt amine complex is 0.4-0.6mg/cm2；
The ratio between quality and the volume of dehydrated alcohol of the cobalt amine complex are (8-12): 1mg/mL, the dehydrated alcohol, distillation
The ratio between volume of water and Nafion reagent is 1:1:0.08.
8. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that described in step (2)
The condition of chronoamperometry are as follows: utilize occasion China CHI 760E electrochemical workstation, be modified with the nickel foam conduct of cobalt amine complex
Working electrode, saturated calomel electrode is as reference electrode, and carbon-point is used as to electrode, and the KOH solution of 1mol/L is electrolyte, timing
The voltage that current method applies is 1.56V.
9. the preparation method of cobalt-based oxygen-separating catalyst according to claim 2, which is characterized in that described in step (2)
Activation time is 20-24h, preferably 22h.
10. oxygen application is analysed in the electro-catalysis of the cobalt-based oxygen-separating catalyst described in claim 1 based on eutectic solvent, it is applied to electricity
It is catalyzed water-splitting and analyses oxygen；Preferably, as water-splitting oxygen-separating catalyst, it is applied to photoelectrocatalysis, basic hydrolysis hydrogen generator
Or APE hydrolyzes battery.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112259750A (en) * | 2020-10-26 | 2021-01-22 | 河北工业大学 | Preparation method and application of polyion liquid functionalized cobalt-nitrogen loaded foamed nickel composite material |
| CN114959783A (en) * | 2022-04-29 | 2022-08-30 | 青岛科技大学 | Co grown in situ in N-C framework 4 Preparation method of N quantum dot electrode material |
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| US20130108802A1 (en) * | 2011-11-01 | 2013-05-02 | Isaiah O. Oladeji | Composite electrodes for lithium ion battery and method of making |
| CN106207187A (en) * | 2016-08-16 | 2016-12-07 | 安徽师范大学 | Hydroxide and nickel foam composite and preparation method thereof |
| CN107308958A (en) * | 2017-06-12 | 2017-11-03 | 首都师范大学 | A kind of oxygen evolution reaction electrochemical catalyst and its preparation and application |
| CN108193227A (en) * | 2016-12-08 | 2018-06-22 | 中国科学院大连化学物理研究所 | Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130108802A1 (en) * | 2011-11-01 | 2013-05-02 | Isaiah O. Oladeji | Composite electrodes for lithium ion battery and method of making |
| CN106207187A (en) * | 2016-08-16 | 2016-12-07 | 安徽师范大学 | Hydroxide and nickel foam composite and preparation method thereof |
| CN108193227A (en) * | 2016-12-08 | 2018-06-22 | 中国科学院大连化学物理研究所 | Oxygen electrode and its preparation and application are analysed in the electro-catalysis of nickel-ferric spinel base |
| CN107308958A (en) * | 2017-06-12 | 2017-11-03 | 首都师范大学 | A kind of oxygen evolution reaction electrochemical catalyst and its preparation and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112259750A (en) * | 2020-10-26 | 2021-01-22 | 河北工业大学 | Preparation method and application of polyion liquid functionalized cobalt-nitrogen loaded foamed nickel composite material |
| CN114959783A (en) * | 2022-04-29 | 2022-08-30 | 青岛科技大学 | Co grown in situ in N-C framework 4 Preparation method of N quantum dot electrode material |
| CN114959783B (en) * | 2022-04-29 | 2023-10-27 | 青岛科技大学 | Co grown in situ in N-C framework 4 Preparation method of N quantum dot electrode material |
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